CN112827360A - Heavy metal adsorption membrane chromatographic ultrafiltration membrane, membrane component and manufacturing method thereof - Google Patents
Heavy metal adsorption membrane chromatographic ultrafiltration membrane, membrane component and manufacturing method thereof Download PDFInfo
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- CN112827360A CN112827360A CN201911156876.4A CN201911156876A CN112827360A CN 112827360 A CN112827360 A CN 112827360A CN 201911156876 A CN201911156876 A CN 201911156876A CN 112827360 A CN112827360 A CN 112827360A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/56—Polyamides, e.g. polyester-amides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
A heavy metal adsorption membrane chromatographic ultrafiltration membrane is characterized in that stock solution of the ultrafiltration membrane adopts at least one of polysulfone, polyether sulfone and PMIA (poly (m-phenyleneisophthalamide)) as polymer resin, and the stock solution is prepared into a hollow fiber membrane and then soaked in chitosan solution. The invention also discloses a membrane component and a preparation method of the ultrafiltration membrane. Compared with the prior artThe invention has the advantages that: the chitosan can be used for adsorbing heavy metal, the glutaraldehyde can help the chitosan to be better adhered to the membrane wires, the heavy metal removal rate of the obtained product can reach more than 95%, and meanwhile, the normal mineral ions Na in water can be treated+、K+、Ca2+、Mg2+And the heavy metal ions can not be removed, so that the conventional mineral ions can be retained in the water purification process to remove the heavy metal ions.
Description
Technical Field
The invention relates to a filtering membrane, belongs to the technical field of water treatment of membranes, and also relates to a membrane module and a preparation method of the membrane.
Background
The existing ultrafiltration membrane generally removes organic matters with relative molecular weight of more than 1000, the ultrafiltration membrane can not remove heavy metal in the purification process of drinking water, and the phenomenon that the drinking water filtered by the ultrafiltration membrane exceeds the standard after long-term drinking exists.
Technical documents for achieving removal of heavy metal particles by modifying ultrafiltration membranes have been disclosed for a long time, and specifically, methods for modifying ultrafiltration membranes mainly include physical methods and chemical methods. The former method is, like the blending method, to physically mix the substance with heavy metal adsorption sites with the film forming material to make the hollow fiber membrane filament, and the blending introduces a large amount of mixture, so that the uniformity of the membrane casting solution is affected, and the formation of the membrane pore structure is affected. The chemical method mainly comprises modification by radiation such as corona, ultraviolet and plasma, and the modification only improves the performance of the material in a short time.
Disclosure of Invention
The first technical problem to be solved by the present invention is to provide an ultrafiltration membrane modified by chitosan to improve the removal rate of heavy metals, in view of the above technical situation.
The second technical problem to be solved by the invention is to provide an ultrafiltration membrane module which is modified by chitosan so as to improve the removal rate of heavy metals.
The third technical problem to be solved by the invention is to provide a preparation method of the ultrafiltration membrane, which improves the removal rate of heavy metals by modifying chitosan.
The technical scheme adopted by the invention for solving the first technical problem is as follows: a heavy metal adsorption membrane chromatographic ultrafiltration membrane is characterized in that stock solution of the ultrafiltration membrane adopts at least one of polysulfone, polyethersulfone and PMIA (poly (m-phenyleneisophthalamide)) as polymer resin, the stock solution is prepared into a hollow fiber membrane and then is soaked by chitosan solution, and the ultrafiltration membrane meets the following conditions:
the external pressure pure water flux is 100-400 (L/M2H bar);
the molecular weight cut-off is between 1 and 10 ten thousand Da.
Furthermore, the removal rate of heavy metal of the ultrafiltration membrane is more than 95%.
Further, the heavy metal is at least one of Cd, Cr, Pb and As.
The technical scheme adopted by the invention for solving the second technical problem is as follows: a membrane component with a heavy metal adsorption membrane chromatographic ultrafiltration membrane is characterized by comprising a shell and the heavy metal adsorption membrane chromatographic ultrafiltration membrane arranged in the shell.
The technical scheme adopted by the invention for solving the third technical problem is as follows: a preparation method of a heavy metal adsorption membrane chromatographic ultrafiltration membrane is characterized by comprising the following steps:
dissolving a polymer resin and an additive in a solvent, wherein the solvent is at least one of DMAC (dimethylacetamide), DMF (dimethylformamide) and NMP (N-methylpyrrolidone), and the additive can adopt the following substances in percentage by weight: 1-10% of polyethylene glycol 1000, 1-10% of polyvinylpyrrolidone K30 or 0.5-5% of LiCl;
secondly, manufacturing a hollow fiber membrane, namely spraying membrane manufacturing stock solution inside and outside a double-layer tubular nozzle at the same time, and soaking the membrane manufacturing stock solution in a coagulating bath containing pure water or salt water to form the hollow fiber membrane;
removing the organic solvent, and removing the organic solvent from the hollow fiber membrane to obtain a nascent hollow fiber membrane;
soaking the nascent hollow fiber membrane in acetic acid solution containing chitosan for the first time, and then adding glutaraldehyde for the second time;
and fifthly, removing redundant organic molecules after soaking to obtain the heavy metal adsorption membrane chromatographic ultrafiltration membrane.
Preferably, the polymer resin is present in the film-forming dope in a concentration of 15 to 35% by weight.
Preferably, the solvent is contained in the film-forming dope in a concentration of 57 to 77% by weight.
Preferably, the concentration of the chitosan is 1-5%.
Preferably, the concentration of the glutaraldehyde is 1-5%.
Preferably, the first soaking in the step (iv) satisfies the following conditions: the soaking temperature is 20-30 ℃, and the soaking time is 1-3 h.
Preferably, the second soaking in the step (iv) satisfies the following conditions: the soaking temperature is 50-80 ℃, and the soaking time is 5-120 min.
Compared with the prior art, the invention has the advantages that: the chitosan molecule contains a large amount of amino groups and can provide a large amount of electrons, heavy metals can provide an empty track in a water body, so that the chitosan molecule can effectively remove heavy metal ions, and glutaraldehyde can perform a crosslinking reaction with hydroxyl groups of the chitosan molecule, so that the chitosan molecule can be well and firmly bonded on the surface and inner holes of the membrane. The heavy metal removal rate of the obtained product can reach more than 95 percent, and the product can simultaneously remove conventional mineral ions Na in water+、K+、Ca2+、Mg2+And the heavy metal ions can not be removed, so that the conventional mineral ions can be retained in the water purification process to remove the heavy metal ions.
Drawings
FIG. 1 is a first photomicrograph of example 2.
FIG. 2 is a second photomicrograph of example 2.
FIG. 3 is a photomicrograph of EXAMPLE 3 III.
FIG. 4 is a cross-sectional view of a specific cross-flow type membrane module.
FIG. 5 is a cross-sectional view of another specific cross-flow type membrane module.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Examples 1 to 9: the polymer membrane material (polysulfone, polyethersulfone and PMIA) is used, the mass percent of the polymer is 15-35%, the mass percent of the solvent is (DMAC, DMF and NMP), the mass percent of the solvent is 57-77%, and the mass percent of the additive PEG1000 polyethylene glycol is 8%. This was stirred for 8 hours and dissolved to prepare a film-forming stock solution. The dope was fed to a spinneret (a double-layer tubular nozzle for producing hollow fibers having a double-layer tube structure) by a constant rate pump and extruded at 4 g/min. The spinneret used had an outer diameter of 0.5mm and an inner diameter of 0.3 mm. Pure water was passed through the internal liquid at a liquid feed rate of 2.0 g/min. The extruded dope for spinning was passed through an air gap of 10mm, put into a coagulating bath of a pure water solution, cooled and solidified, and wound at a winding speed of 20 m/min. The obtained hollow fiber was immersed in water for 24 hours and the solvent was extracted, thereby obtaining a nascent hollow fiber. Soaking a nascent hollow fiber filtering membrane in 2% acetic acid solution containing 2% of chitosan by mass for 2h, adding 2% of glutaraldehyde, soaking the membrane for 30min, raising the temperature to 80 ℃, taking out membrane filaments after fully reacting for 1h, placing the membrane filaments in pure water, and soaking for 24h to obtain the heavy metal adsorption membrane chromatographic ultrafiltration membrane. Micrographs of the ultrafiltration membrane obtained in example 2 are shown in FIG. 1, FIG. 2 and FIG. 3.
Examples 10 to 15: the polymer membrane material PES, the polymer mass is 22%, the solvent is DMAC, the solvent mass% is 70%, and the additive PEG1000 mass% is 8%. This was stirred for 8 hours and dissolved to prepare a film-forming stock solution. The dope was fed to a spinneret (a double-layer tubular nozzle for producing hollow fibers having a double-layer tube structure) by a constant rate pump and extruded at 4 g/min. The spinneret used had an outer diameter of 0.5mm and an inner diameter of 0.3 mm. Pure water was passed through the internal liquid at a liquid feed rate of 2.0 g/min. The extruded dope for spinning was passed through an air gap of 10mm, put into a coagulating bath of a pure water solution, cooled and solidified, and wound at a winding speed of 20 m/min. The obtained hollow fiber was immersed in water for 24 hours and the solvent was extracted, thereby obtaining a nascent hollow fiber. Soaking a nascent hollow fiber filtering membrane in 2% acetic acid solution containing 1-5% of chitosan by mass for 2h, adding 1-5% of glutaraldehyde, soaking the membrane for 30min, raising the temperature to 80 ℃, taking out membrane filaments after full reaction for 1h, placing the membrane filaments in pure water, and soaking for 24h to obtain the heavy metal adsorption membrane chromatographic ultrafiltration membrane.
Example 16: manufacture of cross-flow type assembly
The hollow fiber membranes obtained in example 21 were cut to a length of 180mm, 5000 pieces were bundled, and both ends were plugged with self-made PVC alloy plug glue. A cylindrical tube having an outer diameter of 80mm, an inner diameter of 75mm and a length of 150mm was prepared. Here, in an aluminum material can having the same outer inner diameter as the assembly box and a length of 25mm, a han-high two-component epoxy resin glue potting agent is scraped and filled, one end of the assembly is mounted on the upper portion, and the membrane bundle is extruded from the top to the bottom contacting the aluminum material can. The mixture was left standing for 10 hours in this state, and one end was sealed. After curing, the aluminum can was pulled out while stretching, and the assembly was cut from the epoxy resin for each bundle of films to expose the hollow portion. The end of the other bundle is also sealed and cut in the same manner, so that the hollow portion is exposed at both ends. Both ends of the membrane were covered with covers having inlet and outlet ports and adhered to each other to prepare a cross-flow module having an effective membrane length of 120mm × 5000 membranes.
Example 17: manufacture of cross-flow type assembly
The hollow fiber membrane obtained in example 21 was cut into 360mm lengths, 2500 pieces were bundled, and the holes were plugged with home-made PVC alloy plug glue at both ends. A cylindrical tube having an outer diameter of 80mm, an inner diameter of 75mm and a length of 150mm was prepared. Here, in an aluminum material can having the same outer inner diameter as the assembly box and a length of 25mm, a han-high two-component epoxy resin glue potting agent is scraped and filled, one end of the assembly is mounted on the upper portion, and the membrane bundle is extruded from the top to the bottom contacting the aluminum material can. The mixture was left standing for 10 hours in this state, and one end was sealed. After curing, the aluminum can was pulled out while stretching, and the assembly was cut from the epoxy resin for each bundle of films to expose the hollow portion. The end of the other bundle is also sealed and cut in the same manner, so that the hollow portion is exposed at both ends. Both ends of the membrane were covered with covers having inlet and outlet ports and adhered to each other to prepare a cross-flow module having an effective membrane length of 200mm × 2500 membranes.
The product of example 2 was tested for monovalent and divalent ion rejection rates according to: ultrafiltration membrane and module HY/T112-. The testing device for the ion removal rate of the testing instrument. And (3) testing conditions are as follows: the test medium is distilled water, the water temperature is 25 ℃, the test pressure is 0.1MPa, the solution concentration is 250mg/L, and the operation mode is as follows: and continuously operating for 20min under the test pressure by adopting an external pressure method. The test method comprises the following steps: and testing the conductivity of the raw water and the produced water of the membrane module after the operation is contrasted, and sequentially corresponding to the ion removal rate by the technology. Test objects: magnesium sulfate, calcium chloride, magnesium chloride and sodium chloride. The test results are given in the following table:
test object | Magnesium sulfate | Calcium chloride | Magnesium chloride | Sodium chloride |
Conductivity of raw water (mu s/cm) | 322 | 345 | 301 | 499 |
Conductivity of produced water (mu s/cm) | 322 | 345 | 301 | 499 |
Removal Rate (%) | 0 | 0 | 0 | 0 |
In example 2, the detection results of the cadmium 3-fold national standard limiting concentration of the prepared membrane chromatography ultrafiltration filter element are shown in the following table:
the detection results of the cadmium 5 times of the national standard limiting concentration are shown in the following table:
the results of the detection of the 3-fold international limit concentration of chromium (6-valent) are shown in the following table:
the results of the detection of 5 times the international limit concentration of chromium (6 valent) are shown in the following table:
the detection results of the lead 3 times of the national standard limiting concentration are shown in the following table:
the detection results of the lead 5 times of the national standard limiting concentration are shown in the following table:
the detection results of arsenic 3 times the national standard limiting concentration are shown in the following table:
the detection results of arsenic 5 times the national standard limiting concentration are shown in the following table:
fig. 4 is a specific cross-flow membrane module, and the specific structure comprises a housing 1 and a filter element assembly arranged in the housing 1, wherein a water inlet 11 and a water production port 12 are respectively arranged at two axial ends of the housing 1, a concentrated water outlet 13 is formed in the lateral direction, the filter element assembly comprises a plurality of membrane filaments 2, and adhesive sealing layers 3 are respectively formed at two ends of the membrane filaments.
Fig. 5 shows another specific cross-flow membrane module, which includes a housing 1 and a filter element assembly disposed in the housing 1, wherein a water outlet 12 is formed at one axial end of the housing 1, a water inlet 11 is formed at a lateral side of the housing, and the filter element assembly includes a plurality of membrane filaments 2 and sealant layers 3 formed at two ends of the membrane filaments.
Claims (11)
1. A heavy metal adsorption membrane chromatographic ultrafiltration membrane is characterized in that stock solution of the ultrafiltration membrane adopts at least one of polysulfone, polyethersulfone and polyisophthaloyl metaphenylene diamine as polymer resin, the stock solution is soaked in a chitosan solution after being made into a hollow fiber membrane, and the ultrafiltration membrane meets the following conditions:
the external pressure pure water flux is 100-400 (L/M2H bar);
the molecular weight cut-off is between 1 and 10 ten thousand Da.
2. The heavy metal adsorption membrane chromatographic ultrafiltration membrane according to claim 1, wherein the ultrafiltration membrane has a heavy metal removal rate of 95% or more.
3. The heavy metal adsorption membrane chromatographic ultrafiltration membrane according to claim 2, wherein the heavy metal is at least one of Cd, Cr, Pb and As.
4. A membrane component with the heavy metal adsorption membrane chromatographic ultrafiltration membrane of any one of claims 1-3, which is characterized by comprising a shell and the heavy metal adsorption membrane chromatographic ultrafiltration membrane arranged in the shell.
5. A preparation method of the heavy metal adsorption membrane chromatographic ultrafiltration membrane of any one of claims 1 to 3 is characterized by comprising the following steps:
firstly, preparing a membrane stock solution, namely dissolving polymer resin and an additive in a solvent, wherein the solvent is at least one of dimethylacetamide, dimethylformamide and N-methylpyrrolidone;
secondly, manufacturing a hollow fiber membrane, namely spraying membrane manufacturing stock solution inside and outside a double-layer tubular nozzle at the same time, and soaking the membrane manufacturing stock solution in a coagulating bath containing pure water or salt water to form the hollow fiber membrane;
removing the organic solvent, and removing the organic solvent from the hollow fiber membrane to obtain a nascent hollow fiber membrane;
soaking the nascent hollow fiber membrane in acetic acid solution containing chitosan for the first time, and then adding glutaraldehyde for the second time;
and fifthly, removing redundant organic molecules after soaking to obtain the heavy metal adsorption membrane chromatographic ultrafiltration membrane.
6. The method according to claim 5, wherein the polymer resin is contained in the dope at a concentration of 15 to 35% by weight.
7. The method according to claim 6, wherein the solvent is contained in the dope at a concentration of 57 to 77% by weight.
8. The method according to claim 5, wherein the concentration of the chitosan is 1-5%.
9. The method according to claim 5, wherein the concentration of glutaraldehyde is 1 to 5%.
10. The preparation method according to claim 5, wherein the one-time soaking in the step (iv) satisfies the following conditions: the soaking temperature is 20-30 ℃, and the soaking time is 1-3 h.
11. The preparation method according to claim 5, wherein the second soaking in the step (iv) satisfies the following conditions: the soaking temperature is 50-80 ℃, and the soaking time is 5-120 min.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113880180A (en) * | 2021-09-26 | 2022-01-04 | 宁波方太厨具有限公司 | Preparation method of folding filter element capable of removing heavy metal |
CN113880181A (en) * | 2021-09-26 | 2022-01-04 | 宁波方太厨具有限公司 | Preparation method of filter element capable of removing heavy metal |
CN117185556A (en) * | 2023-09-28 | 2023-12-08 | 宁波众茂杭州湾热电有限公司 | Ultrafiltration purification method for complex water quality of thermal power plant |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113880180A (en) * | 2021-09-26 | 2022-01-04 | 宁波方太厨具有限公司 | Preparation method of folding filter element capable of removing heavy metal |
CN113880181A (en) * | 2021-09-26 | 2022-01-04 | 宁波方太厨具有限公司 | Preparation method of filter element capable of removing heavy metal |
CN117185556A (en) * | 2023-09-28 | 2023-12-08 | 宁波众茂杭州湾热电有限公司 | Ultrafiltration purification method for complex water quality of thermal power plant |
CN117185556B (en) * | 2023-09-28 | 2024-07-30 | 宁波众茂杭州湾热电有限公司 | Ultrafiltration purification method for complex water quality of thermal power plant |
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